Benzene → 4-[4-[[4-[(6-Chloronaphthalen-2-yl)sulfonyl]piperazin-1-yl]carbonyl]phenyl]-1-methylpyridinium iodide

HRID 352901노트

반응식

HRID 352901 반응식
[CH:1]1C=CC=CC=1.[Cl:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[CH:14]=[C:13]([S:18]([N:21]1[CH2:26][CH2:25][N:24]([C:27](=[O:40])[C:28]3[CH:33]=[CH:32][C:31]([C:34]4[CH:39]=[CH:38][N:37]=[CH:36][CH:35]=4)=[CH:30][CH:29]=3)[CH2:23][CH2:22]1)(=[O:20])=[O:19])[CH:12]=[CH:11]2.C[I:42]>CO>[I-:42].[Cl:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][CH:17]=1)[CH:14]=[C:13]([S:18]([N:21]1[CH2:26][CH2:25][N:24]([C:27]([C:28]3[CH:29]=[CH:30][C:31]([C:34]4[CH:39]=[CH:38][N+:37]([CH3:1])=[CH:36][CH:35]=4)=[CH:32][CH:33]=3)=[O:40])[CH2:23][CH2:22]1)(=[O:20])=[O:19])[CH:12]=[CH:11]2

참가 물질

5

반응물 3

HCID 241BenzeneHCID 6328Methyl iodide2회HCID 99572891-[(6-Chloronaphthalen-2-yl)sulfonyl]-4-[4-(pyridin-4-yl)benzoyl]piperazine

생성물 1

HCID 227108464-[4-[[4-[(6-Chloronaphthalen-2-yl)sulfonyl]piperazin-1-yl]carbonyl]phenyl]-1-methylpyridinium iodide수율 58%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a mixed solvent of benzene (10 ml) and methanol (10 ml), 1-[(6-chloronaphthalen-2-yl)sulfonyl]-4-[4-(pyridin-4-yl)benzoyl]piperazine (300 mg) obtained in Example A-1 was dissolved at room temperature, followed by the addition of methyl iodide (1 ml). To the resulting mixture, the same amount of methyl iodide was added three times at intervals of 24 hours, followed by heating under reflux for 4 days. The reaction mixture was distilled under reduced pressure and the residue was washed with methanol, collected by filtration and dried, whereby the title compound (229 mg, 58%) was obtained as a yellow solid.

후처리

  1. dissolutionwas dissolved at room temperature
  2. temperatureby heating
  3. temperatureunder reflux for 4 days
  4. distillationThe reaction mixture was distilled under reduced pressure
  5. washthe residue was washed with methanol
  6. filtrationcollected by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-4a5bc9df6c1543eba5c8cb12c49251a5
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06747023B1

반응 노트

불러오는 중…